CN104415666A - Immersed vacuum membrane distillation concentration method of ethylene glycol solution - Google Patents
Immersed vacuum membrane distillation concentration method of ethylene glycol solution Download PDFInfo
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Abstract
The invention discloses an immersed vacuum membrane distillation concentration method of an ethylene glycol solution, wherein the ethylene glycol solution is concentrated through a gas-dissolving and immersed vacuum membrane distillation technology. The method mainly comprises following steps: (A) pumping the ethylene glycol water solution and a gas to obtain a mixture and pumping the mixture into a water tank; (B) vacuumizing a permeation side of a hollow fiber membrane assembly immersed in the water tank so that condensable gas is condensed at the permeation side to form water and the ethylene glycol solution is intercepted at the water tank; and (C) performing circulating concentration until the mass concentration of the ethylene glycol solution is 70-80% (wt) to obtain a concentrated ethylene glycol solution, thereby achieving concentration and separation of the ethylene glycol solution. By means of the method, the ethylene glycol solution in a process of preparing ethylene glycol from oxirane through a hydration method can be deeply concentrated and dehydrated through membrane distillation and then can be purified in a rectification unit to obtain ethylene glycol. Compared with multiple-effect evaporation, the method is less in equipment investment, is high in treatment efficiency, is low in operation temperature and operation pressure and is low in energy consumption.
Description
Technical field
The present invention relates to the method for concentration of ethylene glycol solution in a kind of hydration of epoxy ethane to prepare ethandiol technique, in particular to a kind of method utilizing film distillation technology concentration ethylene glycol solution, more particularly, a kind of method of air-dissolved, immersion vacuum membrane distillation technology concentration ethylene glycol solution is related to.
Background technology
Current ethylene glycol mostly adopts oxirane Hydrolyze method to produce, obtained dilute solution of ethylene glycol (mass concentration 15%), after downflow type multiple-effect evaporation tower evaporation and concentration, solution concentration reaches and approximates 85% (quality), delivers to thick ethylene glycol storage tank.By the thick ethylene glycol containing 15% (quality) water, dewater in dehydrating tower, arrange aldehyde, tower bottoms still liquid pump, delivers to rectification and purification in purifying ethylene glycol tower, produces high-quality ethylene glycol product.
Due to the boiling point of water, comparatively ethylene glycol boiling point is low, so must first water be evaporated from ethylene glycol, current ethylene glycol solution concentrate and purification mode mainly based on multiple-effect evaporation and rectifying, energy consumption is still very high.
Membrane Materials is the eighties in last century is the hydrophobic membrane technology that seawater desalination is researched and developed, and it adopts microporous hydrophobic membrane, a kind of Aspect of some new membrane processes being driving force with film both sides steam pressure difference.Membrane Materials is the membrane separating process that membrane technology combines with still-process, and its film used is not by the dewatering microporous film of pending solution-wet, and namely only have steam to enter fenestra, liquid can not through fenestra.
Because the inlet temperature of ethylene oxide hydration reaction is 80 ~ 150 DEG C, the outlet temperature about 100 DEG C of mixture after reaction, ethylene glycol solution containing low concentration at normal pressure, the Water Under steam of 80 ~ 95 DEG C under the effect of the both sides vapor partial pressure difference of hydrophobic membrane, water can be realized efficiently be separated with ethylene glycol, compared with multiple-effect evaporation, there is lower operating temperature and energy consumption.
Although what existing pertinent literature related to is a kind of vacuum membrane distillation dewatering by the polyatomic alcohol water solution of Maize Production, but what this patent and document adopted is inner pressed Membrane Materials mode, membrane material is polypropylene (PP), and the film hydrophilic phenomenon caused because polyatomic alcohol water solution concentration raises has appearred in the concentrated later stage.As Chinese patent CN101121639A and document, " vacuum membrane distillation is used for the research that polyatomic alcohol water solution is separated, water technology, 2008, 34 (1), 31 ~ 33 " a kind of vacuum membrane distillation dewatering by the polyatomic alcohol water solution of Maize Production is all related to, involved method adopts distillation device, first polyatomic alcohol water solution is heated to temperature 61 ~ 65 DEG C, then feedstock pump is adopted to join in hollow-fibre membrane by polyatomic alcohol water solution, the vacuum environment of-0.085MPa ~-0.089MPa is formed outside film, thus transmission vapour pressure is formed in film both sides, water inside film in polyatomic alcohol water solution enters outside hollow-fibre membrane through fenestra in vapour form under the effect of steam pressure difference, the cooling condensation Cheng Shui of the condenser system again outside membrane module, collect condensed water, thus realize being concentrated by the dehydration of the polyatomic alcohol water solution of Maize Production.Although this patent and document have employed film distillation technology process polyatomic alcohol water solution, but what this patent and document adopted is inner pressed Membrane Materials mode, membrane material is polypropylene (PP), and the film hydrophilic phenomenon caused because polyatomic alcohol water solution concentration raises has appearred in the concentrated later stage.
Summary of the invention
For the deficiencies in the prior art, the invention discloses a kind of immersion vacuum membrane distillation method for concentration of ethylene glycol solution, aim to provide and a kind ofly adopt air-dissolved, the immersion vacuum membrane distillation technology ethylene glycol solution further in concentrated hydration of epoxy ethane to prepare ethandiol technique, the further moisture removed in recovery ethylene glycol solution, realizes adopting film distillation technology coupling rectification technology to carry out the concentrated purification processes of ethylene glycol solution in hydration of epoxy ethane to prepare ethandiol technique.
The technical solution used in the present invention is:
An immersion vacuum membrane distillation method for concentration for ethylene glycol solution, key step is:
(1) first, glycol water and gas are mixed with certain proportion;
(2) secondly, the gas and liquid mixture of mixed ethylene glycol and gas is pumped into water tank;
(3) last, the per-meate side of the hollow fiber film assembly be immersed in water tank is vacuumized, under vacuum action, gas, water vapour etc. in ethylene glycol mixing wastewater with air liquid are through fenestra, product water can be formed through condenser condenses by condensing body in per-meate side, ethylene glycol solution is then trapped within water tank, obtains ethylene glycol concentration liquid in water tank, so just achieves the concentrated of glycol water and is separated object.
Glycol water water quality characteristic of the present invention is: monoethylene glycol (MEG): 14% (wt), diethylene glycol (DEG): 0.5% (wt), triethylene glycol (TEG): 0.5% (wt), all the other are the glycol water of water.
In the specific implementation, described gas is one or both in nitrogen, air;
In the specific implementation, in step (1), by air dissolved pump by glycol water and the gas and vapor permeation such as air, nitrogen;
In the specific implementation, the described hollow fiber film assembly be immersed in water tank mainly adopts superpower hydrophobic polytetrafluoroethylene (PTFE) (PTFE) hollow fiber hydrophobic membrane assembly;
In the specific implementation, the membrane aperture scope of described polytetrafluoroethylene (PTFE) (PTFE) hollow fiber hydrophobic membrane assembly is 0.15 ~ 0.2 μm;
In the specific implementation, the hollow fiber film assembly of vacuum membrane distillation system adopts immersion operation, be immersed in heating water tank by hollow fiber film assembly, vacuumize formation negative pressure in doughnut fenestra and make water vapour, gas etc. through fenestra, product water can be formed through condenser condenses by condensing body;
In the specific implementation, described polytetrafluoroethylene (PTFE) (PTFE) hollow fiber hydrophobic membrane assembly is two or more sets, interval blocked operation between membrane module; Every special time, the membrane module of operation is out of service, and online bake drying is stand-by;
In the specific implementation, the operating condition being immersed in the hollow fiber film assembly in water tank described in is: glycol water temperature 85 DEG C ~ 100 DEG C; Gas liquid ratio 1.5 ~ 2.5:1; Per-meate side vacuum-0.082 ~-0.092MPa;
In the specific implementation, in water tank, ethylene glycol solution circulation is concentrated to quality of glycol concentration 70% ~ 80% (wt), obtains ethylene glycol concentration liquid.
The essential distinction of the present invention and prior art is, the present invention relates to the method for concentration of ethylene glycol solution in a kind of hydration of epoxy ethane to prepare ethandiol technique.The present invention mainly adopts superpower hydrophobic polytetrafluoroethylene (PTFE) (PTFE) film, take immersion vacuum membrane distillation mode of operation, more particularly, adopt air-dissolved, immersion vacuum membrane distillation mode of operation, concentration is carried out for the ethylene glycol solution in hydration of epoxy ethane to prepare ethandiol technique, simultaneously in order to reduce the hydrophiling problem of ethylene glycol solution to hydrophobic membrane of concentrated later stage higher concentration, molten gas disposal has been carried out in running, and regular intermittently drying membrane module, decrease the hydrophiling problem of ethylene glycol solution to hydrophobic membrane of higher concentration, effectively maintain the hydrophobicity of hydrophobic membrane assembly.
The present invention can obtain following beneficial effect:
1, the reacted ethylene glycol solution of ethylene oxide hydration self has uniform temperature, ethylene oxide hydration reaction outlet temperature about 100 DEG C, and Membrane Materials system generally just can be run at a lower temperature, ethylene glycol solution self used heat therefore can be effectively utilized to carry out the membrane distillation concentration dehydration of ethylene glycol solution;
2, the present invention carries out in the process of ethylene glycol solution thickening at employing vacuum membrane distillation, have employed molten gas disposal, and regular intermittently drying membrane module, decrease the hydrophiling problem of ethylene glycol solution to hydrophobic membrane of higher concentration, effectively maintain the hydrophobicity of hydrophobic membrane assembly;
3, the present invention adopts superpower hydrophobic PTFE hollow-fibre membrane, more effectively reduces the hydrophiling problem of membrane module;
4, adopt the ethylene glycol solution in method concentration hydration of epoxy ethane to prepare ethandiol technique of the present invention, alternative multiple-effect evaporation technology will be expected to, reduce the energy consumption of multiple-effect evaporation technology, improve treatment effeciency.The inventive method is compared with multiple-effect evaporation, has that equipment investment is few, treatment effeciency is high, operating temperature is low, operating pressure is low, low power consumption and other advantages;
5, adopt the method for the invention, the high concentration ethylene glycol solution after membrane distillation concentration dehydration can be carried out rectification and purification process, obtain ethylene glycol.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of immersion vacuum membrane distillation technique in the present invention
In figure: 1-fluid flowmeter, 2-gas flowmeter, 3-air dissolved pump, 4-hollow fiber film assembly, 5-water tank, 6-condenser, 7-vavuum pump.
Detailed description of the invention
Below, by reference to the accompanying drawings and specific embodiment, invention is further described.
Embodiment 1
Process flow diagram is shown in Fig. 1.Figure Central Plains water refers to the ethylene glycol solution in hydration of epoxy ethane to prepare ethandiol technique, its main water quality characteristic is: monoethylene glycol (MEG): 14% (wt), diethylene glycol (DEG): 0.5% (wt), triethylene glycol (TEG): 0.5% (wt), all the other are the glycol water of water.
Membrane module used is polytetrafluoroethylene (PTFE) hollow fiber hydrophobic membrane assembly, and membrane aperture is 0.2 μm.Flow process is as follows:
First, the glycol water of temperature about 90 DEG C is mixed with certain proportion by air dissolved pump and air; Secondly, the gas and liquid mixture of mixed ethylene glycol, air is pumped into water tank; Finally, the per-meate side of the hollow fiber film assembly be immersed in water tank is vacuumized, under vacuum action, gas, water vapour etc. in ethylene glycol mixing wastewater with air liquid are through fenestra, can form product water in per-meate side through condenser condenses by condensing body, ethylene glycol solution is then trapped within water tank, and circulation is concentrated to quality of glycol concentration 80% (wt), ethylene glycol concentration liquid can be obtained, so just achieve the concentrated of glycol water and be separated object.
Concrete operations condition is: glycol water temperature is 90 DEG C, gas liquid ratio 1.5:1, and per-meate side vacuum is-0.082MPa.Under this operating condition, glycol water is concentrated to 80% (wt) from 15% (wt), by detecting the ethylene glycol content in the TOC cubage solution in solution, and amount to into mass fraction investigation concentrated effect, when testing initial, flux of membrane distillation is 14L/m
2about h, when retaining the TOC content in the ethylene glycol concentrated solution of side and being concentrated to 224700mg/L, corresponding ethylene glycol content is 580475mg/L, and the mass fraction amounting to ethylene glycol solution is about 52%, and now flux of membrane distillation is 7.5L/m
2h, when being continued by ethylene glycol solution to be concentrated to 80% (wt), flux of membrane distillation reduces to 4L/m
2about h.In this process, produce the TOC≤5mg/L in water, folding synthesizing glycol≤15mg/L, amounts to into mass fraction≤0.0015% of ethylene glycol solution.
Embodiment 2
Process flow diagram is shown in Fig. 1.Figure Central Plains water refers to the ethylene glycol solution in hydration of epoxy ethane to prepare ethandiol technique, and main water quality characteristic is with embodiment 1.
Membrane module used is polytetrafluoroethylene (PTFE) hollow fiber hydrophobic membrane assembly, and membrane aperture is 0.2 μm.Flow process is as follows:
First, the glycol water of temperature about 85 DEG C is mixed with certain proportion by air dissolved pump and nitrogen; Secondly, the gas and liquid mixture of mixed ethylene glycol, nitrogen is pumped into water tank; Finally, the per-meate side of the hollow fiber film assembly be immersed in water tank is vacuumized, under vacuum action, gas, water vapour etc. in ethylene glycol mixing wastewater with air liquid are through fenestra, can form product water in per-meate side through condenser condenses by condensing body, ethylene glycol solution is then trapped within water tank, and circulation is concentrated to quality of glycol concentration 75% (wt), ethylene glycol concentration liquid can be obtained, so just achieve the concentrated of glycol water and be separated object.
Concrete operations condition is: glycol water temperature is 85 DEG C, gas liquid ratio 2.0:1, and per-meate side vacuum is-0.092MPa.Under this operating condition, glycol water is concentrated to 75% (wt) from 15% (wt), by detecting the ethylene glycol content in the TOC cubage solution in solution, and amount to into mass fraction investigation concentrated effect, when testing initial, flux of membrane distillation is 18L/m
2about h, when retaining the TOC content in the ethylene glycol concentrated solution of side and being concentrated to 224700mg/L, corresponding ethylene glycol content is 580475mg/L, and the mass fraction amounting to ethylene glycol solution is about 52%, and now flux of membrane distillation is 10.5L/m
2h, when being continued by ethylene glycol solution to be concentrated to 75% (wt), flux of membrane distillation reduces to 6.4L/m
2about h.In this process, produce the TOC≤5mg/L in water, folding synthesizing glycol≤15mg/L, amounts to into mass fraction≤0.0015% of ethylene glycol solution.
Embodiment 3
Process flow diagram is shown in Fig. 1.Figure Central Plains water refers to the ethylene glycol solution in hydration of epoxy ethane to prepare ethandiol technique, and main water quality characteristic is with embodiment 1.
Membrane module used is polytetrafluoroethylene (PTFE) hollow fiber hydrophobic membrane assembly, and membrane aperture is 0.15 μm.Flow process is as follows:
First, the glycol water of temperature about 95 DEG C is mixed with certain proportion by air dissolved pump and nitrogen; Secondly, the gas and liquid mixture of mixed ethylene glycol, nitrogen is pumped into water tank; Finally, the per-meate side of the hollow fiber film assembly be immersed in water tank is vacuumized, under vacuum action, gas, water vapour etc. in ethylene glycol mixing wastewater with air liquid are through fenestra, can form product water in per-meate side through condenser condenses by condensing body, ethylene glycol solution is then trapped within water tank, and circulation is concentrated to quality of glycol concentration 80% (wt), ethylene glycol concentration liquid can be obtained, so just achieve the concentrated of glycol water and be separated object.
Concrete operations condition is: glycol water temperature is 95 DEG C, gas liquid ratio 2.5:1, and per-meate side vacuum is-0.082MPa.Under this operating condition, glycol water is concentrated to 80% (wt) from 15% (wt), by detecting the ethylene glycol content in the TOC cubage solution in solution, and amount to into mass fraction investigation concentrated effect, when testing initial, flux of membrane distillation is 16L/m
2about h, when retaining the TOC content in the ethylene glycol concentrated solution of side and being concentrated to 224700mg/L, corresponding ethylene glycol content is 580475mg/L, and the mass fraction amounting to ethylene glycol solution is about 52%, and now flux of membrane distillation is 8.6L/m
2h, when being continued by ethylene glycol solution to be concentrated to 80% (wt), flux of membrane distillation reduces to 4L/m
2about h.In this process, produce the TOC≤5mg/L in water, folding synthesizing glycol≤15mg/L, amounts to into mass fraction≤0.0015% of ethylene glycol solution.
Embodiment 4
Process flow diagram is shown in Fig. 1.Figure Central Plains water refers to the ethylene glycol solution in hydration of epoxy ethane to prepare ethandiol technique, and main water quality characteristic is with embodiment 1.
Membrane module used is polytetrafluoroethylene (PTFE) hollow fiber hydrophobic membrane assembly, and membrane aperture is 0.2 μm.Flow process is as follows:
First, the glycol water of temperature about 100 DEG C is mixed with certain proportion by air dissolved pump and air; Secondly, the gas and liquid mixture of mixed ethylene glycol, air is pumped into water tank; Finally, the per-meate side of the hollow fiber film assembly be immersed in water tank is vacuumized, under vacuum action, gas, water vapour etc. in ethylene glycol mixing wastewater with air liquid are through fenestra, can form product water in per-meate side through condenser condenses by condensing body, ethylene glycol solution is then trapped within water tank, and circulation is concentrated to quality of glycol concentration 80% (wt), ethylene glycol concentration liquid can be obtained, so just achieve the concentrated of glycol water and be separated object.
Concrete operations condition is: glycol water temperature is 100 DEG C, gas liquid ratio 2.0:1, and per-meate side vacuum is-0.085MPa.Under this operating condition, glycol water is concentrated to 80% (wt) from 15% (wt), by detecting the ethylene glycol content in the TOC cubage solution in solution, and amount to into mass fraction investigation concentrated effect, when testing initial, flux of membrane distillation is 20L/m
2about h, when retaining the TOC content in the ethylene glycol concentrated solution of side and being concentrated to 224700mg/L, corresponding ethylene glycol content is 580475mg/L, and the mass fraction amounting to ethylene glycol solution is about 52%, and now flux of membrane distillation is 11L/m
2h, when being continued by ethylene glycol solution to be concentrated to 80% (wt), flux of membrane distillation reduces to 6L/m
2about h.In this process, produce the TOC≤5mg/L in water, folding synthesizing glycol≤15mg/L, amounts to into mass fraction≤0.0015% of ethylene glycol solution.
Embodiment 5
Process flow diagram is shown in Fig. 1.Figure Central Plains water refers to the ethylene glycol solution in hydration of epoxy ethane to prepare ethandiol technique, and main water quality characteristic is with embodiment 1.
Membrane module used is polytetrafluoroethylene (PTFE) hollow fiber hydrophobic membrane assembly, and membrane aperture is 0.2 μm.Flow process is as follows:
First, the glycol water of temperature about 100 DEG C is mixed with certain proportion by air dissolved pump and air; Secondly, the gas and liquid mixture of mixed ethylene glycol, air is pumped into water tank; Finally, the per-meate side of the hollow fiber film assembly be immersed in water tank is vacuumized, under vacuum action, gas, water vapour etc. in ethylene glycol mixing wastewater with air liquid are through fenestra, can form product water in per-meate side through condenser condenses by condensing body, ethylene glycol solution is then trapped within water tank, and circulation is concentrated to quality of glycol concentration 70% (wt), ethylene glycol concentration liquid can be obtained, so just achieve the concentrated of glycol water and be separated object.
Concrete operations condition is: glycol water temperature is 100 DEG C, gas liquid ratio 1.8:1, and per-meate side vacuum is-0.092MPa.Under this operating condition, glycol water is concentrated to 70% (wt) from 15% (wt), by detecting the ethylene glycol content in the TOC cubage solution in solution, and amount to into mass fraction investigation concentrated effect, when testing initial, flux of membrane distillation is 23L/m
2about h, when retaining the TOC content in the ethylene glycol concentrated solution of side and being concentrated to 224700mg/L, corresponding ethylene glycol content is 580475mg/L, and the mass fraction amounting to ethylene glycol solution is about 52%, and now flux of membrane distillation is 13L/m
2h, when being continued by ethylene glycol solution to be concentrated to 70% (wt), flux of membrane distillation reduces to 9.8L/m
2about h.In this process, produce the TOC≤5mg/L in water, folding synthesizing glycol≤15mg/L, amounts to into mass fraction≤0.0015% of ethylene glycol solution.
The foregoing is only better possible embodiments of the present invention, not thereby limit to the scope of the claims of the present invention, therefore the equivalent structure change that every utilization description of the present invention and accompanying drawing content are done, be all contained in protection scope of the present invention.
Claims (9)
1. an immersion vacuum membrane distillation method for concentration for ethylene glycol solution, key step is:
(1) first, glycol water and gas are mixed with certain proportion;
(2) secondly, the gas and liquid mixture of mixed ethylene glycol and gas is pumped into water tank;
(3) last, the per-meate side of the hollow fiber film assembly be immersed in water tank is vacuumized, product water can be formed in per-meate side through condenser condenses by condensing body, in water tank, obtain ethylene glycol concentration liquid.
2. the immersion vacuum membrane distillation method for concentration of ethylene glycol solution according to claim 1, it is characterized in that, described glycol water water quality characteristic is: monoethylene glycol (MEG) 14% (wt), diethylene glycol (DEG) 0.5% (wt), triethylene glycol (TEG) 0.5% (wt), all the other are the glycol water of water.
3. the immersion vacuum membrane distillation method for concentration of ethylene glycol solution according to claim 1 or 2, is characterized in that, described in be immersed in the hollow fiber film assembly in water tank operating condition be: glycol water temperature 85 DEG C ~ 100 DEG C; Gas liquid ratio 1.5 ~ 2.5:1; Per-meate side vacuum-0.082 ~-0.092MPa.
4. the immersion vacuum membrane distillation method for concentration of ethylene glycol solution according to claim 1 or 2, is characterized in that, described gas is one or both in nitrogen, air.
5. the immersion vacuum membrane distillation method for concentration of ethylene glycol solution according to claim 1 or 2, is characterized in that, in step (1), by air dissolved pump by glycol water and gas and vapor permeation.
6. the immersion vacuum membrane distillation method for concentration of ethylene glycol solution according to claim 1 or 2, it is characterized in that, the described hollow fiber film assembly be immersed in water tank adopts superpower hydrophobic polytetrafluoroethylene (PTFE) (PTFE) hollow fiber hydrophobic membrane assembly.
7. the immersion vacuum membrane distillation method for concentration of ethylene glycol solution according to claim 6, it is characterized in that, the membrane aperture scope of described polytetrafluoroethylene (PTFE) (PTFE) hollow fiber hydrophobic membrane assembly is 0.15 ~ 0.2 μm.
8. the immersion vacuum membrane distillation method for concentration of ethylene glycol solution according to claim 6, it is characterized in that, described polytetrafluoroethylene (PTFE) (PTFE) hollow fiber hydrophobic membrane assembly is two or more sets, interval blocked operation between membrane module.
9. the immersion vacuum membrane distillation method for concentration of ethylene glycol solution according to claim 1 or 2, is characterized in that, in water tank, ethylene glycol solution circulation is concentrated to quality of glycol concentration 70% ~ 80% (wt), obtains ethylene glycol concentration liquid.
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CN104817128A (en) * | 2015-04-17 | 2015-08-05 | 中国科学院生态环境研究中心 | Device and method for dissolved gas film deamination |
CN106348393A (en) * | 2016-09-30 | 2017-01-25 | 新奥科技发展有限公司 | Membrane distillation system and membrane distillation method |
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CN102408140A (en) * | 2010-09-25 | 2012-04-11 | 中国石油化工股份有限公司 | Method for removing and recycling volatile alcohol organic matters in water |
CN102417210A (en) * | 2010-09-28 | 2012-04-18 | 中国石油化工股份有限公司 | Immersed vacuum membrane distillation plant and sewage treatment technology using the same |
CN103193295A (en) * | 2012-01-06 | 2013-07-10 | 中国石油化工股份有限公司 | Immersed dissolved gas vacuum membrane distillation water processing method |
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CN101327407A (en) * | 2007-06-20 | 2008-12-24 | 天津工业大学 | Apparatus and method for evaporating and concentrating liquid |
CN101121639A (en) * | 2007-07-13 | 2008-02-13 | 天津大学 | Membrane distillation dehydration method for polyatomic alcohol water solution produced from corn |
CN102408140A (en) * | 2010-09-25 | 2012-04-11 | 中国石油化工股份有限公司 | Method for removing and recycling volatile alcohol organic matters in water |
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